ASTM D1552-07
(Test Method)Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)
Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)
SIGNIFICANCE AND USE
This test method provides a means of monitoring the sulfur level of various petroleum products and additives. This knowledge can be used to predict performance, handling, or processing properties. In some cases the presence of sulfur compounds is beneficial to the product and monitoring the depletion of sulfur can provide useful information. In other cases the presence of sulfur compounds is detrimental to the processing or use of the product.
SCOPE
p id="s00002">1.1 This test method covers three procedures for the determination of total sulfur in petroleum products including lubricating oils containing additives, and in additive concentrates. This test method is applicable to samples boiling above 177°C (350°F) and containing not less than 0.06 mass % sulfur. Two of the three procedures use iodate detection; one employing an induction furnace for pyrolysis, the other a resistance furnace. The third procedure uses IR detection following pyrolysis in a resistance furnace.
1.2 Petroleum coke containing up to 8 mass % sulfur can be analyzed.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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An American National Standard
Designation:D1552–07
Standard Test Method for
1
Sulfur in Petroleum Products (High-Temperature Method)
This standard is issued under the fixed designation D 1552; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* 3. Summary of Test Method
1.1 This test method covers three procedures for the deter- 3.1 Iodate Detection System—The sample is burned in a
mination of total sulfur in petroleum products including stream of oxygen at a sufficiently high temperature to convert
lubricating oils containing additives, and in additive concen- about 97 % of the sulfur to sulfur dioxide. A standardization
trates. This test method is applicable to samples boiling above factor is employed to obtain accurate results. The combustion
177°C(350°F)andcontainingnotlessthan0.06mass %sulfur. products are passed into an absorber containing an acid
Two of the three procedures use iodate detection; one employ- solution of potassium iodide and starch indicator. A faint blue
ing an induction furnace for pyrolysis, the other a resistance color is developed in the absorber solution by the addition of
furnace. The third procedure uses IR detection following standard potassium iodate solution. As combustion proceeds,
pyrolysis in a resistance furnace. bleaching the blue color, more iodate is added. The amount of
1.2 Petroleum coke containing up to 8 mass % sulfur can be standard iodate consumed during the combustion is a measure
analyzed. of the sulfur content of the sample.
1.3 The values stated in SI units are to be regarded as the 3.2 IR Detection System—The sample is weighed into a
standard. The values given in parentheses are for information special ceramic boat which is then placed into a combustion
only. furnace at 1371°C (2500°F) in an oxygen atmosphere. Most
1.4 This standard does not purport to address all of the sulfur present is combusted to SO which is then measured
2
safety concerns, if any, associated with its use. It is the with an infrared detector after moisture and dust are removed
responsibility of the user of this standard to establish appro- by traps. A microprocessor calculates the mass percent sulfur
priate safety and health practices and determine the applica- from the sample weight, the integrated detector signal and a
bility of regulatory limitations prior to use. predeterminedcalibrationfactor.Boththesampleidentification
number and mass percent sulfur are then printed out. The
2. Referenced Documents
calibration factor is determined using standards approximating
2
2.1 ASTM Standards: the material to be analyzed.
D 1193 Specification for Reagent Water
4. Significance and Use
D 1266 Test Method for Sulfur in Petroleum Products
(Lamp Method) 4.1 This test method provides a means of monitoring the
D 4057 Practice for Manual Sampling of Petroleum and sulfur level of various petroleum products and additives. This
Petroleum Products knowledge can be used to predict performance, handling, or
D 6299 Practice for Applying Statistical Quality Assurance processing properties. In some cases the presence of sulfur
Techniques to Evaluate Analytical Measurement System compounds is beneficial to the product and monitoring the
Performance depletion of sulfur can provide useful information. In other
D 6792 Practice for Quality System in Petroleum Products cases the presence of sulfur compounds is detrimental to the
and Lubricants Testing Laboratories processing or use of the product.
5. Interferences
1
This test method is under the jurisdiction of ASTM Committee D02 on
5.1 For the iodate systems, chlorine in concentrations less
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
than 1 mass % does not interfere. The IR system can tolerate
D02.03 on Elemental Analysis.
somewhat higher concentrations. Nitrogen when present in
Current edition approved Dec. 1, 2007. Published January 2008. Originally
approved in 1958. Last previous edition approved in 2003 as D 1552–03.
excessof0.1mass %mayinterferewiththeiodatesystems;the
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
extent of such interference may be dependent on the type of
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
nitrogen compound as well as the combustion conditions.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Nitrogen does not interfere with the IR system. The alkali and
*A Summary of Changes section appears at th
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
An American National Standard
Designation:D1552–03 Designation:D1552–07
Standard Test Method for
1
Sulfur in Petroleum Products (High-Temperature Method)
This standard is issued under the fixed designation D 1552; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope*
1.1 This test method covers three procedures for the determination of total sulfur in petroleum products including lubricating
oils containing additives, and in additive concentrates. This test method is applicable to samples boiling above 177°C (350°F) and
containing not less than 0.06 mass % sulfur.Two of the three procedures use iodate detection; one employing an induction furnace
for pyrolysis, the other a resistance furnace. The third procedure uses IR detection following pyrolysis in a resistance furnace.
1.2 Petroleum coke containing up to 8 mass % sulfur can be analyzed.
1.3
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D 1266 Test Method for Sulfur in Petroleum Products (Lamp Method)
D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D 6299 Practice for Applying Statistical Quality Assurance Techniques to Evaluate Analytical Measurement System
Performance
D 6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories
3. Summary of Test Method
3.1 Iodate Detection System—The sample is burned in a stream of oxygen at a sufficiently high temperature to convert about
97 % of the sulfur to sulfur dioxide.Astandardization factor is employed to obtain accurate results. The combustion products are
passed into an absorber containing an acid solution of potassium iodide and starch indicator.Afaint blue color is developed in the
absorber solution by the addition of standard potassium iodate solution. As combustion proceeds, bleaching the blue color, more
iodate is added. The amount of standard iodate consumed during the combustion is a measure of the sulfur content of the sample.
3.2 IR Detection System—The sample is weighed into a special ceramic boat which is then placed into a combustion furnace
at 1371°C (2500°F) in an oxygen atmosphere. Most sulfur present is combusted to SO which is then measured with an infrared
2
detectoraftermoistureanddustareremovedbytraps.Amicroprocessorcalculatesthemasspercentsulfurfromthesampleweight,
theintegrateddetectorsignalandapredeterminedcalibrationfactor.Boththesampleidentificationnumberandmasspercentsulfur
are then printed out. The calibration factor is determined using standards approximating the material to be analyzed.
4. Significance and Use
4.1 This test method provides a means of monitoring the sulfur level of various petroleum products and additives. This
knowledgecanbeusedtopredictperformance,handling,orprocessingproperties.Insomecasesthepresenceofsulfurcompounds
is beneficial to the product and monitoring the depletion of sulfur can provide useful information. In other cases the presence of
sulfur compounds is detrimental to the processing or use of the product.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
Elemental Analysis.
Current edition approved March 10, 2003. Published April 2003. Originally approved in 1958. Last previous edition approved in 2001 as D1552–01.
Current edition approved Dec. 1, 2007. Published January 2008. Originally approved in 1958. Last previous edition approved in 2003 as D 1552–03.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard.
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